WO2008062632A1 - Appareil de production de trichlorosilane - Google Patents

Appareil de production de trichlorosilane Download PDF

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Publication number
WO2008062632A1
WO2008062632A1 PCT/JP2007/070805 JP2007070805W WO2008062632A1 WO 2008062632 A1 WO2008062632 A1 WO 2008062632A1 JP 2007070805 W JP2007070805 W JP 2007070805W WO 2008062632 A1 WO2008062632 A1 WO 2008062632A1
Authority
WO
WIPO (PCT)
Prior art keywords
gas
trichlorosilane
reaction vessel
heat transfer
transfer body
Prior art date
Application number
PCT/JP2007/070805
Other languages
English (en)
Japanese (ja)
Inventor
Mitsutoshi Narukawa
Yuji Shimizu
Original Assignee
Mitsubishi Materials Corporation
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Priority claimed from JP2007268617A external-priority patent/JP5160181B2/ja
Application filed by Mitsubishi Materials Corporation filed Critical Mitsubishi Materials Corporation
Priority to US12/312,471 priority Critical patent/US8221691B2/en
Priority to CN2007800429212A priority patent/CN101535180B/zh
Publication of WO2008062632A1 publication Critical patent/WO2008062632A1/fr

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B33/00—Silicon; Compounds thereof
    • C01B33/08—Compounds containing halogen
    • C01B33/107—Halogenated silanes
    • C01B33/1071—Tetrachloride, trichlorosilane or silicochloroform, dichlorosilane, monochlorosilane or mixtures thereof

Definitions

  • the present invention relates to a trichlorosilane production apparatus that converts tetrachlorosilane to trichlorosilane.
  • SiHCl 3 is converted by reacting tetrachlorosilane (SiCl: silicon tetrachloride) with hydrogen.
  • Patent Document 1 discloses a double chamber design in which a reaction chamber surrounded by a heating element has an outer chamber and an inner chamber formed by two concentric tubes. Has been.
  • a reactor has been proposed in which a supply gas of hydrogen and tetrachlorosilane is supplied to the reaction chamber from below, and a reaction product gas is discharged from the bottom of the reaction chamber.
  • a heating element which is a heater formed of carbon or the like, generates heat when energized, and heats the inside of the reaction chamber from the outside to heat the tube. The gas is heated and reacted while passing through a cylindrical path formed concentrically between these tubes.
  • Patent Document 1 Japanese Patent No. 3781439
  • the conversion reaction from tetrachlorosilane to trichlorosilane has a higher conversion efficiency as the temperature range in the conversion furnace is wider.
  • the above prior art has a problem that the conversion efficiency is extremely low because the high temperature region is limited to the region heated by the radiant heat from the heating element outside the reaction chamber.
  • the present invention has been made in view of the above-described problems, and an object of the present invention is to provide a trichlorosilane production apparatus capable of efficiently heating a supply gas to provide a reaction.
  • the trichlorosilane production apparatus of the present invention includes a reaction vessel in which a supply gas containing tetrachlorosilane and hydrogen is supplied to generate a reaction product gas containing trichlorosilane and hydrogen chloride, and the inside of the reaction vessel
  • a heat transfer body that is formed of a material having a melting point of at least 1400 ° C. and that has a gap through which gas can flow, and a heating mechanism that heats the heat transfer body in the reaction vessel. It is characterized by being.
  • a heat transfer body having a melting point of at least 1400 ° C. is filled in a reaction vessel, and is heated by radiant heat and conduction heat transfer from a heating mechanism.
  • the contact area between the supply gas and the heat transfer body is increased by the gap of the heat transfer body, so that the heat can be efficiently generated.
  • the supply gas since the supply gas is widely distributed through the gap, the supply gas can be heated by the entire heat transfer body.
  • the reason why the melting point of the heat transfer body exceeds 1400 ° C is that it may be heated to 1400 ° C in order to carry out the conversion reaction, so that the solid state can be maintained at a high temperature. is there.
  • the reaction vessel has a gas supply port for introducing the supply gas into the reaction vessel, and a gas guide for leading the reaction product gas out of the reaction vessel.
  • the supply gas introduced from the supply port flows in a fixed direction from the one end side to the gas outlet port on the other end side in the filling portion. Therefore, the supply gas and the reaction product gas can flow easily without stagnation in the filling section, and the conversion reaction can be performed efficiently.
  • the trichlorosilane production apparatus of the present invention is characterized in that the heat transfer body is composed of a plurality of agglomerates or molded block bodies! /. A gap in the heat transfer body can be effectively secured by the plurality of agglomerates or block bodies.
  • the trichlorosilane production apparatus of the present invention is characterized in that a plurality of irregularities are formed on the surface of the agglomerates or molded block bodies. That is, in this trichlorosilane manufacturing apparatus, a lump having a plurality of irregularities on the surface or a molded block body is adopted, so that the contact area with the supply gas can be increased, and heating can be performed more efficiently. You can use fi S, S.
  • the trichlorosilane production apparatus of the present invention is characterized in that the heat transfer body is any one of polycrystalline silicon, silicon carbide, and carbon whose surface is coated with silicon carbide. That is, in this trichlorosilane manufacturing apparatus, since any one of heat transfer members of polycrystalline silicon, silicon carbide (SiC), or carbon whose surface is coated with silicon carbide is employed, impurities are hardly generated and thermal conductivity is increased. High heating efficiency can be obtained.
  • the invention's effect is any one of polycrystalline silicon, silicon carbide (SiC), or carbon whose surface is coated with silicon carbide.
  • the reaction container is filled with a heat transfer element that is formed of a material having a melting point that exceeds at least 1400 ° C. and that has a gap that allows gas to flow therethrough. And heated.
  • the contact area with the supply gas increases, and efficient heating becomes possible. Therefore, an efficient conversion reaction can be obtained with high heating efficiency, and the conversion rate to trichlorosilane can be improved.
  • FIG. 1 is a simplified cross-sectional view showing a first embodiment of a trichlorosilane production apparatus according to the present invention.
  • FIG. 2 is an enlarged perspective view of essential parts showing a state in which block bodies are stacked in a second embodiment of the trichlorosilane manufacturing apparatus according to the present invention.
  • FIG. 3A is a plan view of the block bodies stacked in the second embodiment.
  • FIG. 3B is a side view of the block bodies stacked in the second embodiment when viewed from the inside of the radius.
  • a supply gas containing tetrachlorosilane and hydrogen is supplied into the interior to generate a reaction product gas containing trichlorosilane and hydrogen chloride.
  • Reaction vessel 1 a large number of agglomerates 2 having a melting point of at least 1400 ° C filled in reaction vessel 1 and heated by radiant heat and conduction heat transfer, and reaction vessel V is provided with a heating mechanism 3 arranged around 1 and heating the agglomerates 2 in the reaction vessel 1 by radiant heat and conduction heat transfer.
  • the reaction vessel 1 includes a gas supply port la for introducing a supply gas therein, a gas outlet port lb for deriving a reaction product gas to the outside, and a filling unit 4 filled with a large number of agglomerates 2. ing.
  • a gas supply port la is disposed below (one end side) of the filling portion 4 and a gas outlet port lb is disposed above (on the other end side).
  • the agglomerate 2 is one of high-purity polycrystalline silicon, silicon carbide, and carbon whose surface is coated with silicon carbide. In particular, those having a plurality of irregularities on the surface are employed.
  • the size and filling amount of the agglomerates 2 are appropriately set according to the flow rate of the supply gas to be circulated, the size (filling capacity) of the filling portion 4, and the like. Then, by filling a large number of the granule 2, the filling portion 4 is formed in a state in which the gap portions 2 a through which gas can flow between the respective granule 2 are intricately assembled.
  • the filling unit 4 is a partition plate 5 provided with a certain space from the bottom of the reaction vessel 1. Formed on top.
  • a gas supply port la is provided in the space between the partition plate 5 and the bottom of the reaction vessel 1 so that supply gas is introduced.
  • the partition plate 5 is formed with a plurality of gas inflow holes 5a smaller than the outer diameter of the agglomerates 2! /. The supply gas flows into the filling part 4 from these gas inflow holes 5a.
  • the gas supply port la is connected to a supply source (not shown) of a supply gas.
  • the supply gas flowing in from the gas inflow hole 5a flows upward in the gap 2a between the granule 2 in the filling unit 4. At this time, since it is heated while being in contact with the surface of the agglomerate 2, it reacts to become a reaction product gas. This reaction product gas is finally led out from the upper gas outlet lb force.
  • the heating mechanism 3 includes a heater unit 3a that is a heating element disposed around the reaction vessel 1 so as to surround the reaction vessel 1, and a heater unit 3a that is connected to a lower portion of the heater unit 3a and allows a current to flow through the heater unit 3a. And an electrode portion 3b.
  • the electrode portion 3b is connected to a power source (not shown).
  • the heating mechanism 3 performs heating control so that the agglomerate 2 in the reaction vessel 1 has a temperature in the range of 800 ° C to 1400 ° C. If the temperature of the agglomerate 2 is set to 1200 ° C or higher, the conversion rate to trichlorosilane is improved. Alternatively, disilanes may be introduced into the supply gas and the silanes may be taken out.
  • a large number of agglomerates 2 having a melting point exceeding 1400 ° C. are filled in the reaction vessel 1 and heated by the radiant heat and conduction heat transfer of the heating mechanism 3.
  • the gap 2a formed between the granulates 2 increases the contact area between the supply gas having many gaps and the granule 2 and can be efficiently heated.
  • the supply gas since the supply gas is widely distributed through the gap 2a between the agglomerates 2, the supply gas can be heated in the entire filling unit 4.
  • the contact area with the supply gas can be increased, and heating can be performed more efficiently.
  • any agglomerate 2 of polycrystalline silicon, silicon carbide, or carbon whose surface is coated with silicon carbide is employed, impurities are hardly generated. Together with this, the thermal conductivity is high, and high heating efficiency can be obtained.
  • carbon whose surface is coated with silicon carbide is used as the agglomerate 2
  • hydrogen, chlorosilane, and hydrogen chloride in carbon, supply gas, and reaction product gas are used.
  • methane, methylchlorosilane, silicon carbide, etc. from being produced and becoming impurities.
  • the gas supply port la is arranged below the filling unit 4 and the gas outlet port 1b is arranged above the filling unit 4, the supply gas introduced from the gas supply port la is contained in the filling unit 4. Flows in a fixed direction from the lower side force to the upper gas outlet lb. Therefore, the supply gas and the reaction product gas can easily flow in the filling section 4 without stagnation. As a result, the conversion reaction can be performed efficiently.
  • the direction of gas flow is indicated by arrows.
  • FIGS. 2, 3A and 3B a second embodiment of the trichlorosilane production apparatus according to the present invention will be described below with reference to FIGS. 2, 3A and 3B.
  • the same components as those described in the above embodiments are denoted by the same reference numerals, and the description thereof is omitted.
  • the difference between the second embodiment and the first embodiment is that, in the first embodiment, the filling section 4 is filled with a plurality of agglomerates 2 as a heat transfer body, whereas the second embodiment is different from the second embodiment.
  • the molded block body 22 is used as a heat transfer body, and the block body 22 is lined up and filled in the filling section 4. That is, in the trichlorosilane manufacturing apparatus according to the second embodiment, as shown in FIGS. 2 and 3A, a plurality of block bodies 22 molded in a substantially arc shape are provided in a plurality of annular shapes having different diameters in the filling portion 4. They are arranged and stacked.
  • the block body 22 includes a substantially arc-shaped main body portion 22a and a convex portion 22b protruding from the inside of the main body portion 22a.
  • the block bodies 22 are arranged in a plurality of annular shapes in contact with each other in the bottomed cylindrical filling portion 4. It is further stacked on top of it. Thus, a space 22c through which gas flows is formed between the convex portions 22b of each block body 22. In this case, when a plurality of the block bodies 22 are arranged in an annular shape and are stacked, as shown in FIG.
  • the upper and lower block bodies 22 are arranged so as to be shifted from each other in the circumferential direction, and the convex portions 22b are Is set so that they do not match.
  • the upper and lower convex portions 22b are shifted and arranged so that the upper and lower gap portions 22c are continuous while meandering.
  • the supply gas and the reaction product gas are circulated through the meandering continuous gap 22c.
  • the second embodiment a large number of gaps are formed in the filling portion 4 between each other. Since the molded block bodies 22 are lined up side by side, it is easy to increase the temperature as in the first embodiment, and the contact area between the supply gas and the block body 22 is increased. Therefore, it can power to heat efficiently. Further, since the supply gas spreads widely through the gap portion 22c between the block bodies 22, the supply gas can be heated in the entire filling portion 4.
  • the supply gas is introduced from below the filling unit 4 and the reaction product gas is led out from above.
  • gas may be introduced and derived from a different direction.
  • the supply gas may be introduced from one side in the horizontal direction of the filling unit 4 and the reaction product gas may be derived from the other side in the horizontal direction.
  • the force is transmitted by one molded block body that can be filled in the filling portion of the force reaction vessel, each of which constitutes a heat transfer body by a plurality of agglomerates or a plurality of block bodies.
  • a molded block body in which a void portion is formed from the surface to the inside by a combination structure of columnar portions or plate-like portions may be used as the heat transfer body.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Silicon Compounds (AREA)

Abstract

L'invention concerne un appareil de production de trichlorosilane comprenant un récipient réactionnel dans lequel un gaz d'apport contenant du tétrachlorosilane et de l'hydrogène est fourni pour produire un gaz de produit réactionnel contenant du trichlorosilane et du chlorure d'hydrogène ; un corps de transfert thermique qui est chargé dans le récipient réactionnel et constitué d'au moins un matériau ayant un point de fusion supérieur à 1400 °C, tout en ayant un espace dans lequel un gaz peut passer ; et un mécanisme de chauffage pour chauffer le corps de transfert thermique dans le récipient réactionnel.
PCT/JP2007/070805 2006-11-21 2007-10-25 Appareil de production de trichlorosilane WO2008062632A1 (fr)

Priority Applications (2)

Application Number Priority Date Filing Date Title
US12/312,471 US8221691B2 (en) 2006-11-21 2007-10-25 Apparatus for producing trichlorosilane
CN2007800429212A CN101535180B (zh) 2006-11-21 2007-10-25 三氯硅烷制造装置

Applications Claiming Priority (4)

Application Number Priority Date Filing Date Title
JP2006314896 2006-11-21
JP2006-314896 2006-11-21
JP2007-268617 2007-10-16
JP2007268617A JP5160181B2 (ja) 2006-11-21 2007-10-16 トリクロロシラン製造装置

Publications (1)

Publication Number Publication Date
WO2008062632A1 true WO2008062632A1 (fr) 2008-05-29

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ID=39429571

Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/JP2007/070805 WO2008062632A1 (fr) 2006-11-21 2007-10-25 Appareil de production de trichlorosilane

Country Status (1)

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WO (1) WO2008062632A1 (fr)

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS4847500A (fr) * 1971-10-21 1973-07-05
JPS56169119A (en) * 1980-05-27 1981-12-25 Mitsubishi Metal Corp Manufacture of trichlorosilane
JPS62123011A (ja) * 1985-11-25 1987-06-04 Koujiyundo Silicon Kk トリクロルシランの製造方法およびその装置
JPH07232910A (ja) * 1994-01-28 1995-09-05 Hemlock Semiconductor Corp テトラクロロシランの水素添加法

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS4847500A (fr) * 1971-10-21 1973-07-05
JPS56169119A (en) * 1980-05-27 1981-12-25 Mitsubishi Metal Corp Manufacture of trichlorosilane
JPS62123011A (ja) * 1985-11-25 1987-06-04 Koujiyundo Silicon Kk トリクロルシランの製造方法およびその装置
JPH07232910A (ja) * 1994-01-28 1995-09-05 Hemlock Semiconductor Corp テトラクロロシランの水素添加法

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